Structural and catalytic properties of Ti–MCM-41 synthesised at room temperature up to high Ti content

A study of the pore structural properties and catalytic activity of MCM-41 containing titanium, prepared by direct synthesis at ambient temperature and pressure, using tetraethoxysilane, titanium alcoxides, cationic surfactants and ammonia is presented. The influence of different metal sources (titanium ethoxide, isopropoxide or n-butoxide), alcohols (ethanol or propan-2-ol), metal content (2 ⩽ Si/Ti ⩽ 100) and surfactants (tetra-, hexa- or octadecyltrimethylammonium bromide) is considered. The materials were characterised by X-ray diffraction, nitrogen adsorption at 77 K and diffuse reflectance UV–Vis spectroscopy. The catalytic activity was evaluated in the model reaction of oxidation of cyclohexene with anhydrous tert-butylhydroperoxide, for representative samples. It is concluded that this method allows the preparation in a short period of time of well structured and catalytically active Ti–MCM-41. Down to Si/Ti = 10 the materials have high pore volumes and very uniform pore size, with highest conversion and excellent selectivity demonstrated in the compositional range 30 ⩽ Si/Ti ⩽ 100, corresponding to materials containing predominantly isolated and tetracoordinated Ti. The increase in Ti content to Si/Ti ratios of 10 and 5 implied a reduction both in conversion and selectivity, although the MCM-41 structure was still observed for Si/Ti = 2.